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1.
用毛细管区带电泳 -电化学检测法测定了黄芩及其制剂中黄芩素和黄芩甙的含量。研究了电极电位、电解液酸度和浓度、电泳电压及进样时间等对电泳的影响 ,得到了较为优化的测定条件。以直径为300μm的碳圆盘电极为检测电极 ,电极电位为0.90V(vsSCE) ,在100mmol/L硼酸盐缓冲液(pH9.0)中 ,上述两组分在8min内完全分离。黄芩素和黄芩甙浓度与电泳峰电流分别在5.0×10 -7~1.0×10 -3mol/L和1.0×10 -6~1.0×10 -3mol/L范围内呈良好线性 ,检出限分别为2.24×10 -7mol/L和5.48×10 -7mol/L。7次测定分别含5.0×10 -4mol/L黄芩素和黄芩甙试样溶液 ,峰高的相对标准偏差分别为3.53%和4.03%。  相似文献   

2.
黄芩甙的线性扫描伏安法测定研究   总被引:1,自引:0,他引:1  
研究了黄芩甙在多壁碳纳米管修饰电极上的伏安行为。结果表明 ,该修饰电极对黄芩甙产生较强的吸附催化作用 ,催化电流与黄芩甙浓度在 1 .0× 1 0 - 7~ 6.0×1 0 - 5mol·L- 1范围内呈线性关系。利用本法测定了中药黄芩中的黄芩甙的含量 ,效果良好  相似文献   

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黄芩甙在玻碳电极上的电化学行为及其应用   总被引:1,自引:0,他引:1  
用线性扫描伏安法(LSV)、循环伏安法(CV)和常规脉冲伏安法(NPV)等多种电化学方法研究了黄芩甙在玻碳电极上的电化学行为,并建立了尿样和血清样品中黄芩甙的微分脉冲伏安(DPV)测定法。实验结果表明:黄芩甙在玻碳电极上的吸附符合Frumkin吸附等温式,吸附自由能为-35.01kJ mol。采用整体电解法求得电极反应电子数为2,并结合Nernst方程式推导了反应机理。黄芩甙在玻碳电极上预富集后,在4.20×10-10~1.05×10-5mol L范围内分段呈线性关系,对5.60×10-7mol L黄芩甙溶液连续6次测定的RSD=2.0%,检出限为2.8×10-10mol L。  相似文献   

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高效毛细管电泳法分离测定黄芩复方制剂中的黄芩甙   总被引:4,自引:0,他引:4  
韩凤梅  程智勇  杨新  陈勇 《色谱》2000,18(3):280-280
 建立了清开灵口服液和双黄连口服液中黄芩甙定量分析的高效毛细管电泳方法。选择毛细管区带电泳分离模式,以40mmol/L硼砂缓冲液(pH9.0)为电泳介质,未涂层石英毛细管(50μmi.d.×39.5cm,有效分离长度34.8cm)为分离通道,对硝基苯甲酸为内标,压力进样(68.95kPa×s),17kV恒压电泳(25℃),于285nm下分离分析两种黄芩复方制剂中的黄芩甙。实验结果表明,黄芩甙可在15min内与其它成分得到很好的分离,在10~640mg/L范围内定量分析。加样回收率分别为:清开灵口服液(100.31±1.98)%,双黄连口服液(100.60±2.36)%。方法简便、快速、准确,重现性好,可用于黄芩复方制剂。  相似文献   

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黄芩甙的极谱催化波研究及应用   总被引:9,自引:0,他引:9  
在 0 .2 4mol/L混合酸 NaOH(Britton Robinson) (pH 2 .0 ) -8× 1 0 -3 mol/LKIO3 支持电解质中 ,黄芩甙产生一极谱催化波 ,峰电位为 -1 .2 0V(vs.SCE)。该波的一阶导数峰峰电流与黄芩甙浓度在 1×1 0 -7~ 3× 1 0 -6mol/L范围内呈线性关系 (r=0 .9988)。用该法测定了三黄片中黄芩甙的含量。该催化波是有机化合物极谱催化波的一种新类型—缔合 /平行催化波。IO-3 有双重作用 :( 1 )IO-3 作为配位体与吸附在电极表面的质子化黄芩甙形成离子对缔合物 ,引起峰电位的负移 ;( 2 )IO-3 及其还原中间体作为氧化剂氧化黄芩甙羰基经单电子单质子还原产生的自由基 ,产生了极谱催化波  相似文献   

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建立了毛细管电泳法测定中药复方制剂双黄连口恨液中黄芩甙元、黄芩甙、绿原酸和咖啡酸的方法,通过研究缓冲溶液pH和浓度、分离电压、进样时间和有饥添加剂的影响优化了分析条件在优化的条件下,20min内实现了4种物质的良好分离黄芩甙元、黄芩甙、绿原酸和咖啡酸峰高和质量浓度分别在0.05~1.50、0.06~1.20、0.02~0.50和0.02~0.50g/L范围内呈良好线性;俭出限分别为0.015、0.020、0.004、0.004g/L基于迁移时间和峰高的重复性分别为:黄芩甙元,1.70%和3.94%;黄芩甙,1.60%和3.63%;绿原酸,1.60%和2.05%;咖啡酸,1.51%和2.83%通过分析实际样品并做加标回收实验验证了该方法的可行性。  相似文献   

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黄芩素在一定的电位范围内具有明显的电化学信号,Al3+的加入对于黄芩素的电信号具有显著的抑制作用,且氧化峰电流的降低值ΔI p与Al3+浓度呈良好的线性关系,基于此建立了方波伏安法测定Al3+的新方法。通过对支持电解质、黄芩素的浓度、加入顺序等条件进行优化,发现在2.0×10-8~5.0×10-7mol/L和5.0×10-7~8.0×10-6mol/L范围内,ΔI p与Al3+浓度成正比,检出限为2.2×10-8mol/L;并对油条中的Al3+进行了检测。同时,利用循环伏安法、紫外光谱法等初步探讨了黄芩素与Al3+的作用机理,研究发现黄芩素在玻碳电极上发生了2电子2质子的电化学转移行为,且其电极氧化过程受到吸附作用控制;加入Al3+后,二者生成了一种新型络合物,导致黄芩素的电化学活性显著降低。  相似文献   

8.
银黄冲剂中黄芩甙和绿原酸的毛细管电泳分离分析   总被引:8,自引:0,他引:8  
杨新  韩凤梅  程智勇  陈勇 《色谱》1999,17(6):573-575
摘要:用毛细管电泳法分离并测定了银黄冲剂中黄芩甙和绿原酸。以对硝基苯甲酸为内标,未涂层融硅毛细管(50μmi.d.,370μmo.d.,总长47cm,有效分离长度40cm)为分离通道,25mmol/L硼砂缓冲液(pH8.5)为电泳介质,17kPa·s压力进样,25kV恒压电泳,310nm检测。黄芩甙和绿原酸线性范围分别为160~960mg/L(r=0.9993,RSD=1.76%~2.33%)和80~960mg/L(r=0.9989,RSD=1.07%~2.51%),加入回收率:黄芩甙为(102.09±1  相似文献   

9.
通过系统优化缓冲溶液pH、工作电压和进样时间等因素的影响建立了毛细管电泳法分析清开灵口服液和银黄片中黄芩甙和绿原酸的方法。黄芩甙和绿原酸的峰高和浓度分别在0.06~1.20和0.02~0.50 g·L-1浓度范围内呈良好线性。基于迁移时间和峰高的相对标准偏差黄芩甙为1.60%和2.63%;绿原酸为1.48%和2.65%。根据3倍噪音法得出黄芩甙和绿原酸的检出限分别为0.020 g·L-1和0.004 g·L-1,实际样品分析的相对标准偏差均小于4%,利用银黄片做加标回收试验,黄芩甙和绿原酸的回收率分别为97.6%和97.3%。  相似文献   

10.
齐莉  周蓉 《化学分析计量》1999,8(3):10-11,21
应用胶束电动毛细管色谱技术分离黄芩中主要的黄酮类有效成分并进行分析,确定它们分别是:黄芩甙、黄芩素、汉黄芩甙、汉黄芩素、木蝴蝶素A及木蝴 A-7-D-葡萄糖甙。缓冲液由20mmol/LSDS、20mmol/LL的磷酸三氮钠及25mmol/L的硼砂组成,溶液的P来7.24。在胶束电动车管色谱分析中,黄芩中的主要黄酮类有铲成分在15min内即可达到基线分离,并且能对黄芩甙进行定量分析,笔者还讨论了表面  相似文献   

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We review our research on the synthesis and study of the physical and biological properties of furyl- and thienylgermatranes and -silatranes.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 725–732, June, 1992.  相似文献   

14.
The use of the insect cell/baculovirus expression system for producing recombinant proteins of bacterial, plant, insect, and mammalian origin has become widespread. The popularity of this eukaryotic expression system is due to many factors, including (1) potentially high protein expression levels, (2) ease and speed of genetic engineering, (3) ability to accommodate large DNA inserts, (4) protein processing similar to higher eukaryotic cells (e.g., mammalian cells), and (5) ease of insect cell growth (e.g., suspension growth). The following review of the literature discusses two engineering aspects of recombinant protein synthesis by insect cell cultures: bioreactor scale-up and insect cell line selection. Following this review patent abstracts and additional literature pertaining to expression of recombinant proteins in insect cell culture are listed.  相似文献   

15.
多环芳二酐型聚酯亚胺膜的透气性能李悦生,丁孟贤,徐纪平(浙江大学高分子科学与工程研究所,杭州,310027)(中国科学院长春应用化学研究所)关键词聚醚酰亚胺,聚酯酰亚胺,膜,透气性通常的聚酰亚胺加工性能较差,在芳环二酐的苯环间引入醚键等柔性基团后,其...  相似文献   

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微量元素与疾病诊断治疗的研究现状及展望   总被引:8,自引:0,他引:8  
对国内外微量元素与疾病的关系及其诊断治疗的研究现状及研究动向进行了综述,包括:微量元素与地方病、癌肿、心血管病、糖尿病、眼病、神经系统病等。参考文献72篇。  相似文献   

19.
Poly-p-ethylacrylophenone (PPEtAP) and poly-p-chloroacrylophenone (PPClAP) and their copolymers with styrene (PEtAP/S) and (PClAP/S) and with methyl methacrylate (PEtAP/MMA) and (PClAP/MMA) were prepared. Quantum yields of main-chain scissions at 366 nm at room temperature in benzene solution are of the same order as those of the unsubstituted polyacrylophenone and its copolymers. Substitution with chlorine and ethyl group in the para position compared to the unsubstituted polyacrylophenone and its copolymers leads to an increase of the lifetime for the n–π* excited triplet state, as is evident from the measured quenching constants of photolysis. The low-temperature emission spectra of the copolymers are similar to the spectra of the model compounds in a polymer film. For the homopolymer, however, the character of the emission spectrum changes considerably.  相似文献   

20.
A total of 35 trace and minor elements including some of environmental significance were determined in each of a selection of 15 Chinese and 6 Canadian thermal coals and their ashes by using the SLOWPOKE-2 nuclear reactor facility of the University of Toronto. The concentrations and distributions of these constituents among the coals and their combustion products (viz. ash and volatile matter) are presented together with an interpretation of their significance in relation to the large scale combustion of these coals as thermal fuels in industrialized countries such as China and Canada. The detailed results showed wide variations in trace impurity concentrations (up to a factor of 100 and more) among the coals studied with few large differences between those of Chinese and Canadian origin except that the rare earths, Sc, Th, U, I, and Se were much higher in the former, other halogens, As and Na were lower. Values for elemental enrichment factors (EF) relative to normal crustal abundances indicated that only As(EF=13), Br(5.7), I(16), S(230), Sb(11) and Se(320) were appreciably enriched in coal. During static ashing at 750°C most of the halogens, S and Se were volatilized whereas most other inorganic constituents were highly retained and concentrated in the ash by factors of 6 to 11.  相似文献   

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